CN104745132B - A kind of outdoor paster lamp bead epoxide-resin glue and preparation method thereof - Google Patents
A kind of outdoor paster lamp bead epoxide-resin glue and preparation method thereof Download PDFInfo
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- CN104745132B CN104745132B CN201510115670.2A CN201510115670A CN104745132B CN 104745132 B CN104745132 B CN 104745132B CN 201510115670 A CN201510115670 A CN 201510115670A CN 104745132 B CN104745132 B CN 104745132B
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- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 30
- 239000003292 glue Substances 0.000 title claims abstract description 29
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000011324 bead Substances 0.000 title claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 238000005538 encapsulation Methods 0.000 claims abstract description 13
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 5
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 5
- 239000007822 coupling agent Substances 0.000 claims abstract description 5
- 239000004611 light stabiliser Substances 0.000 claims abstract description 5
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 4
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000010792 warming Methods 0.000 claims description 16
- 239000004593 Epoxy Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 claims description 12
- 150000004702 methyl esters Chemical class 0.000 claims description 9
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- YBHBEZSZXFLQMW-UHFFFAOYSA-N [dimethoxy(phenyl)silyl]methanamine Chemical compound CO[Si](CN)(OC)C1=CC=CC=C1 YBHBEZSZXFLQMW-UHFFFAOYSA-N 0.000 claims description 8
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 8
- 238000005292 vacuum distillation Methods 0.000 claims description 8
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical class CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 6
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- 239000001361 adipic acid Substances 0.000 claims description 3
- 235000011037 adipic acid Nutrition 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims 4
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000032683 aging Effects 0.000 abstract description 3
- 230000001590 oxidative effect Effects 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 18
- -1 diisoamyl diene Chemical class 0.000 description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 6
- OSWPMRLSEDHDFF-UHFFFAOYSA-N methyl salicylate Chemical group COC(=O)C1=CC=CC=C1O OSWPMRLSEDHDFF-UHFFFAOYSA-N 0.000 description 6
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000004224 protection Effects 0.000 description 5
- 150000003254 radicals Chemical class 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 3
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000003379 elimination reaction Methods 0.000 description 3
- 239000003925 fat Substances 0.000 description 3
- 235000019253 formic acid Nutrition 0.000 description 3
- 229960001047 methyl salicylate Drugs 0.000 description 3
- 150000002924 oxiranes Chemical class 0.000 description 3
- 235000019260 propionic acid Nutrition 0.000 description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical group OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 125000003545 alkoxy group Chemical group 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 2
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical class OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 2
- LTVUCOSIZFEASK-MPXCPUAZSA-N (3ar,4s,7r,7as)-3a-methyl-3a,4,7,7a-tetrahydro-4,7-methano-2-benzofuran-1,3-dione Chemical compound C([C@H]1C=C2)[C@H]2[C@H]2[C@]1(C)C(=O)OC2=O LTVUCOSIZFEASK-MPXCPUAZSA-N 0.000 description 1
- KILURZWTCGSYRE-LNTINUHCSA-K (z)-4-bis[[(z)-4-oxopent-2-en-2-yl]oxy]alumanyloxypent-3-en-2-one Chemical compound CC(=O)\C=C(\C)O[Al](O\C(C)=C/C(C)=O)O\C(C)=C/C(C)=O KILURZWTCGSYRE-LNTINUHCSA-K 0.000 description 1
- LQZZUXJYWNFBMV-UHFFFAOYSA-N 1-dodecanol group Chemical class C(CCCCCCCCCCC)O LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 1
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 1
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 description 1
- 229910015900 BF3 Inorganic materials 0.000 description 1
- 229930185605 Bisphenol Natural products 0.000 description 1
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- HECLRDQVFMWTQS-UHFFFAOYSA-N Dicyclopentadiene Chemical compound C1C2C3CC=CC3C1C=C2 HECLRDQVFMWTQS-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Substances FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 1
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- KEVMYFLMMDUPJE-UHFFFAOYSA-N diisoamyl Natural products CC(C)CCCCC(C)C KEVMYFLMMDUPJE-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 description 1
- KWUZCAVKPCRJPO-UHFFFAOYSA-N n-ethyl-4-(6-methyl-1,3-benzothiazol-2-yl)aniline Chemical compound C1=CC(NCC)=CC=C1C1=NC2=CC=C(C)C=C2S1 KWUZCAVKPCRJPO-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
- 229920006009 resin backbone Polymers 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- HWCKGOZZJDHMNC-UHFFFAOYSA-M tetraethylammonium bromide Chemical compound [Br-].CC[N+](CC)(CC)CC HWCKGOZZJDHMNC-UHFFFAOYSA-M 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Landscapes
- Adhesives Or Adhesive Processes (AREA)
- Epoxy Resins (AREA)
Abstract
The present invention relates to a kind of epoxide-resin glue, and in particular to a kind of outdoor paster lamp bead epoxide-resin glue and preparation method thereof.The outdoor paster lamp bead epoxide-resin glue of the present invention, the glue is made up of two kinds of components of A, B, it is characterized in that, wherein A glue is made up of epoxy resin, antioxidant, light stabilizer and coupling agent；B glue is made up of curing agent, accelerator, polyalcohol, blue agent.The present invention is the epoxide-resin glue for outdoor paster lamp bead.Have that bonding force is strong, thermal oxidative aging is strong, moisture resistance is good, the advantages of ultraviolet-resistent property is strong.Outdoor paster lamp bead encapsulation glue is especially suitable for, is adapted to industrialized production.
Description
Technical field
The present invention relates to a kind of epoxide-resin glue, and in particular to a kind of outdoor paster lamp bead epoxide-resin glue and its preparation
Method.
Background technology
Due to LED have electric light transformation efficiency height, environmental protection, long lifespan, low operating voltage, small volume, generate heat less, brightness
The advantages of high, light beam concentrates stable, therefore it is widely used in the fields such as radiating light source, illumination and display.Used to reduce LED
During light because of scattering loss, that is, to chip carry out mechanical protection, it need to be packaged.Because it makes in open air for a long time
Must possess higher light transmittance, refractive index with, LED encapsulation material, excellent resistant of high or low temperature and protection against the tide, solvent resistant, color inhibition,
Ultraviolet aging resistance and other optics, chemical property.
Current LED pasters encapsulating material mainly uses organic siliconresin, but the high refractive index organic silicon resin of domestic production
Cementability and stability are poor, therefore domestic market is occupied by Dow corning and Japanese SHIN-ETSU HANTOTAI etc. always.Common bisphenol type epoxy
Resin high temperature resistant, color inhibition and ultra-violet resistance are poor, therefore are less applied to LED and encapsulate.
Country someone studied the envelope that silane coupler modified cycloaliphatic epoxy resin is used as high-powered LED lamp at present
Glue is filled, the CN102703008A patent applications as disclosed in Chinese patent disclose a kind of packaging plastic for great power LED,
But, the glue has the shortcomings that production cost is high, viscosity is high, anti-moisture performance is not good, is not suitable for outdoor paster lamp bead.
The content of the invention
The present invention new is used for outdoor SMD lamp to solve the above-mentioned problems in the prior art there is provided a kind of
Epoxide-resin glue of pearl and preparation method thereof.
The outdoor paster lamp bead epoxide-resin glue of the present invention, the glue is made up of two kinds of components of A, B, and wherein component A is by ring
Oxygen tree fat, antioxidant, light stabilizer and coupling agent composition；B component is made up of curing agent, accelerator, polyalcohol, blue agent.
The preferred scheme of the present invention is that the weight ratio of component A and B component is 1:0.9-1.0, and component A is by by weight
The following material composition of part ratio：Organic-silicon-modified cycloaliphatic epoxy resin 10-15
Preferably, B component by ratio by weight following material composition：
Organic-silicon-modified cycloaliphatic epoxy resin of the present invention is POSS structure silsesquioxane resins；It is preferred that by following
Method is made：By aminomethyl phenyl dimethoxysilane, phenyltrimethoxysila,e, 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl front three
The aqueous hydrochloric acid solution of TMOS 0.1% is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to
The accessory substance that 120-130 DEG C of vacuum distillation elimination reaction is produced, produces organic-silicon-modified cycloaliphatic epoxy resin.
The preferred scheme of the present invention is that described cycloaliphatic epoxy resin is double (2,3 epoxy cyclopentyl) ether, 3,4- ring
Epoxide -6- methylcyclohexyls formic acid -3 ', 4 '-epoxy radicals -6 '-methylcyclohexyl methyl esters, vinyl cyclic ethylene diepoxide,
3,4- expoxycyclohexyl formic acid -3 ', 4 '-expoxycyclohexyl methyl esters, diisoamyl diene diepoxide, adipic acid two (3,
4- epoxy radicals -6- methylcyclohexyls methyl esters), the one or more in bicyclopentadiene diepoxide.
The preferred scheme of the present invention is that the antioxidant is 2,6- di-tert-butyl-4-methy phenols, four [β-(3,5- bis-
Tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester,
One or more in the double Lauryl Alcohol esters of triphenyl phosphite, the monooctyl ester of phosphorous acid three, thio-2 acid.
The preferred scheme of the present invention is that the light stabilizer is Methyl Salicylate, the 2- (2 ˊ-ˊ of hydroxyl-5-methyl
Phenyl) BTA, the one or more in 2-hydroxy-4-n-octoxybenzophenone.
The preferred scheme of the present invention is that the coupling agent is glycidol ether alkoxy silane.
The preferred scheme of the present invention is that the curing agent is methylhexahydrophthalic anhydride, methyl hexahydro O-phthalic
In acid anhydrides and methyl tetrahydrophthalic anhydride mixture, methylhexahydrophthalic anhydride and methylnadic anhydride mixture
One or more.
The present invention preferred scheme be, the accelerator be tetramethyl amine bromide, tetraethylammonium bromide, 2-methylimidazole,
One or more in 2-ethyl-4-methylimidazole, aluminium acetylacetonate, boron trifluoride amine complex.
The preferred scheme of the present invention is, the polyalcohol is glycerine, 1,6- hexylene glycols, neopentyl glycol, polyethylene glycol, poly-
One or more in propane diols.
The present invention also provides the preparation method of outdoor paster lamp bead epoxide-resin glue, comprises the steps：
1) preparation of component A：Be 10-15 organic-silicon-modified cycloaliphatic epoxy resin by weight, 40-45 fat
Ring race epoxy resin, 40-45 bisphenol-A epoxy resins, 0.1-3 antioxidant, 0.1-3 light stabilizer, 0.5-4
Coupling agent is put into reactor in proportion, and 1-2h, froth breaking, encapsulation are stirred in 80-100 DEG C；
2) preparation of B component：Be 92-96 curing agent by weight, 0.1-3 accelerator, 0.5-3 it is polynary
Alcohol, 0.001-0.01 tune blue agent are proportionally added into reactor, and 1-2h, froth breaking, encapsulation are stirred in 70-90 DEG C.
3) it is 1 according to weight ratio by component A and B component:0.9-1.0 proportioning, it is well mixed to be solidified, wherein in
125-130 DEG C first solidifies 0.5-1.5 hours, solidifies 3~5 hours after 130-150 DEG C, produces outdoor paster lamp bead asphalt mixtures modified by epoxy resin
Fat glue.
The present invention carries out modification by copolymerization to epoxy resin, a kind of modifying epoxy resin by organosilicon is synthesized, by being aggregated in ring
In oxygen resin backbone after embedded Si-O-Si keys, the epoxy resin cure after organic-silicon-modified, with bonding force is strong, heat resistanceheat resistant oxygen
Aging is strong, moisture resistance is good, the advantages of ultraviolet-resistent property is strong.Outdoor paster lamp bead encapsulation glue is especially suitable for, is adapted to industry metaplasia
Production.
Embodiment
The invention will be described further by the following examples, of the invention to help understanding, but the protection model of the present invention
Enclose and be not limited in these embodiments.
Embodiment one
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% benzene
Base trimethoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid
The aqueous solution is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation
The accessory substance that elimination reaction is produced.
(2) preparation of component A：By weight than the organic-silicon-modified cycloaliphatic epoxy resin for 13%, 44% adipic acid
Two (3,4- epoxy radicals -6- methylcyclohexyls methyl esters), 40% bisphenol-A epoxy resin, 1% 2,6- di-t-butyls -4-
Methylphenol, 1% Methyl Salicylate, 1% γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane is in proportion
Put into reactor, 1-2h, froth breaking are stirred in 80-100 DEG C.
(3) preparation of B component：By weight than methyl hexahydrophthalic anhydride for 96%, 1% 2-methylimidazole, 2.99%
Polyethylene glycol, 0.01% tune blue agent are proportionally added into reactor, and 1-2h, froth breaking are stirred in 70-90.
(4) component of A, B two presses 1：0.94 it is well mixed solidified, wherein in 125-130 DEG C first solidification 0.5-1.5 it is small
When, solidify 3~5 hours after 130-150 DEG C, produce outdoor paster lamp bead epoxide-resin glue.
Embodiment two
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% benzene
Base trimethoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid
The aqueous solution is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation and takes off
The accessory substance produced except reaction.
(2) preparation of component A：By weight than organic-silicon-modified cycloaliphatic epoxy resin, the 45% 3,4- rings for 12%
Epoxide hexahydrobenzoid acid -3 ', 4 '-expoxycyclohexyl methyl esters, 40% bisphenol-A epoxy resin, the four of 1% [β-(3,5-
Di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 1% 2-hydroxy-4-n-octoxybenzophenone, 1% γ-
(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is put into reactor in proportion, and 1-2h, froth breaking are stirred in 80-100 DEG C.
(3) preparation of B component：By weight than the methyl hexahydrophthalic anhydride for 96%, 1% 4 bromide, 2.99%
Polypropylene glycol, 0.01% tune blue agent be proportionally added into reactor, in 70-90 stir 1-2h, froth breaking.
(4) component of A, B two presses 1：0.96 it is well mixed solidified, wherein in 125-130 DEG C first solidification 0.5-1.5 it is small
When, solidify 3~5 hours after 130-150 DEG C, produce outdoor paster lamp bead epoxide-resin glue.
Embodiment three
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% benzene
Base trimethoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid
The aqueous solution is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation and takes off
The accessory substance produced except reaction.
(2) preparation of component A：By weight for 10% organic-silicon-modified cycloaliphatic epoxy resin, the 3 of 45%,
4- expoxycyclohexyls formic acid -3 ', 4 '-expoxycyclohexyl methyl esters, 40.8% bisphenol-A epoxy resin, 0.1% β -
(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester, 0.1% 2-hydroxy-4-n-octoxybenzophenone, 4%
Glycidol ether alkoxy silane put into proportion in reactor, in 80-100 DEG C stir 1-2h, froth breaking, encapsulation；
(3) preparation of B component：By weight for 96% methylhexahydrophthalic anhydride, 3% 2- ethyls-
4-methylimidazole, 0.999% 1,6- hexylene glycols, 0.001% tune blue agent are proportionally added into reactor, in 70-90
DEG C stirring 1-2h, froth breaking, encapsulation.
(4) it is 1 according to weight ratio by component A and B component:0.9 proportioning, it is well mixed to be solidified, wherein in 125-
130 DEG C first solidify 0.5-1.5 hours, solidify 3~5 hours after 130-150 DEG C, produce outdoor paster lamp bead epoxy resin
Glue.
Example IV
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% benzene
Base trimethoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid
The aqueous solution is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation and takes off
The accessory substance produced except reaction
(2) preparation of component A：By weight than organic-silicon-modified cycloaliphatic epoxy resin, the 42% 3,4- rings for 15%
Epoxide hexahydrobenzoid acid -3 ', 4 '-expoxycyclohexyl methyl esters, 40% bisphenol-A epoxy resin, the four of 1% [β-(3,5-
Di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 1% 2-hydroxy-4-n-octoxybenzophenone, 1% γ-
(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is put into reactor in proportion, and 1-2h, froth breaking are stirred in 80-100 DEG C.
(3) preparation of B component：By weight than the methyl hexahydrophthalic anhydride for 96%, 1% 4 bromide, 2.99%
Polypropylene glycol, 0.01% tune blue agent be proportionally added into reactor, in 70-90 stir 1-2h, froth breaking.
(4) component of A, B two presses 1：0.95 proportioning, it is well mixed to be solidified, wherein first solidifying 0.5- in 125-130 DEG C
1.5 hours, solidify 3~5 hours after 130-150 DEG C, produce outdoor paster lamp bead epoxide-resin glue.
Embodiment five
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% benzene
Base trimethoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid
The aqueous solution is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation and takes off
The accessory substance produced except reaction.
(2) preparation of component A：By weight part ratio for 12 parts organic-silicon-modified cycloaliphatic epoxy resin, 42 parts it is double (2,
3 epoxy cyclopentyls) ether, 40 parts of bisphenol-A epoxy resins, 0.2 part of 2,6 di tert butyl 4 methyl phenol, 3 parts
Methyl Salicylate, 4 parts of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane are put into reactor in proportion,
1-2h, froth breaking, encapsulation are stirred in 80-100 DEG C；
(3) preparation of B component：Methylhexahydrophthalic anhydride, 0.9 part of tetraethyl by weight for 95 parts
Ammonium bromide, 2.2 parts of neopentyl glycol, 0.005 part of tune blue agent are proportionally added into reactor, and 1- is stirred in 70-90 DEG C
2h, froth breaking, encapsulation.
(4) it is 1 according to weight ratio by component A and B component:0.9 proportioning, it is well mixed to be solidified, wherein in 125-
130 DEG C first solidify 0.5-1.5 hours, solidify 3~5 hours after 130-150 DEG C, produce outdoor paster lamp bead epoxy resin
Glue.
Embodiment six
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% benzene
Base trimethoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid
The aqueous solution is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation
The accessory substance that elimination reaction is produced
(2) preparation of component A：Organic-silicon-modified cycloaliphatic epoxy resin, oneself of 41 parts by weight for 15 parts
Diacid two (3,4- epoxy radicals -6- methylcyclohexyls methyl esters), 44 parts of bisphenol-A epoxy resins, 1.7 parts of phosphorous acid three are pungent
Ester, 1.6 parts of 2-hydroxy-4-n-octoxybenzophenone, 2.6 parts of γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane
Put into proportion in reactor, 1-2h, froth breaking, encapsulation are stirred in 80-100 DEG C；
(3) preparation of B component：Methylhexahydrophthalic anhydride, 1.4 parts of acetyl by weight for 94.6 parts
Acetone aluminium, 2.5 parts of glycerine, 0.009 part of tune blue agent are proportionally added into reactor, and 1-2h is stirred in 70-90 DEG C,
Froth breaking, encapsulation.
(4) it is 1 according to weight ratio by component A and B component:1 proportioning, it is well mixed to be solidified, wherein in 125-130
DEG C first solidify 0.5-1.5 hour, after 130-150 DEG C of solidification 3~5 hours, produce outdoor paster lamp bead epoxide-resin glue.
The product of the embodiment of the present invention, after testing：1. outward appearance is transparency liquid, no isolation, gel and particle, each component face
Aberration is different substantially；2. existing phenyl polysiloxane structure in the organic-silicon-modified cycloaliphatic epoxy resin synthesized, molecular structure, also has
Alicyclic epoxy structural, solidfied material has good high-low temperature resistant and UVResistant effect；3. impact strength is more than 12.8KJ/m2,
Bending strength is more than 14J；4. glass transition temperature is more than 423.15K；5. -40 DEG C (30min) → 100 DEG C (30min) circulations 600
Secondary, thermal shock is unchanged；6. three Reflow Solderings (260 DEG C of peak temperature, time 10s) packaging plastic is crossed without coming off and xanthochromia is existing
As；7. it is hot and humid：70 DEG C, 90% relative humidity, 100 DEG C of digestion 1h of red ink or soak at room temperature 30 days, no infiltration.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, it is simple
Change, should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (1)
1. a kind of outdoor paster lamp bead epoxide-resin glue, the glue is made up of two kinds of components of A, B, it is characterized in that, wherein component A by
Epoxy resin, antioxidant, light stabilizer and coupling agent composition；B component is by curing agent, accelerator, polyalcohol, blue agent group
Into, it is characterized in that, it is made up of following steps：
(1) organic-silicon-modified cycloaliphatic epoxy resin is prepared：By 15% aminomethyl phenyl dimethoxysilane, 10% phenyl three
Methoxy silane, 60% 2- (3,4- 7-oxa-bicyclo[4.1.0s base) ethyl trimethoxy silanes and 15% 0.1% hydrochloric acid are water-soluble
Liquid is put into reactor in proportion, is warming up to 90-120 DEG C of reaction backflow 4-5h, is warming up to 120-130 DEG C of vacuum distillation removing anti-
The accessory substance that should be produced；
(2) preparation of component A：Organic-silicon-modified cycloaliphatic epoxy resin, 41 parts of adipic acid by weight for 15 parts
Two (3,4- epoxy radicals -6- methylcyclohexyls methyl esters), 44 parts of bisphenol-A epoxy resins, 1.7 parts of the monooctyl ester of phosphorous acid three,
1.6 parts of 2-hydroxy-4-n-octoxybenzophenone, 2.6 parts of γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane are pressed
Ratio is put into reactor, and 1-2h, froth breaking, encapsulation are stirred in 80-100 DEG C；
(3) preparation of B component：Methylhexahydrophthalic anhydride, 1.4 parts of acetylacetone,2,4-pentanedione by weight for 94.6 parts
Aluminium, 2.5 parts of glycerine, 0.009 part of tune blue agent are proportionally added into reactor, are stirred 1-2h in 70-90 DEG C, are disappeared
Bubble, encapsulation；
(4) it is 1 according to weight ratio by component A and B component:1 proportioning, it is well mixed to be solidified, wherein in 125-130 DEG C of elder generation
Solidification 0.5-1.5 hours, solidifies 3~5 hours after 130-150 DEG C, produces outdoor paster lamp bead epoxide-resin glue.
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| CN105238315B (en) * | 2015-11-20 | 2018-02-06 | 烟台德邦先进硅材料有限公司 | A kind of silicon-modified epoxy packaging plastic |
| CN105384914A (en) * | 2015-12-18 | 2016-03-09 | 无锡创达新材料股份有限公司 | High-temperature-resistant ultraviolet-resistant epoxy resin prepolymer and preparation method thereof |
| RU2760687C2 (en) | 2017-06-09 | 2021-11-29 | Хексион Инк. | Epoxy resin systems for composites |
| CN109825232A (en) * | 2019-02-27 | 2019-05-31 | 华南理工大学 | A kind of epoxy encapsulant for LED and preparation method thereof |
| CN110746918A (en) * | 2019-10-30 | 2020-02-04 | 惠州市鑫惠利光电材料有限公司 | Low-light-attenuation LED epoxy packaging adhesive |
| CN111334247A (en) * | 2020-04-17 | 2020-06-26 | 南京智聚科技咨询有限公司 | Packaging adhesive for full-spectrum LED lamp |
| CN111334232A (en) * | 2020-04-28 | 2020-06-26 | 东莞市恒尔朗实业有限公司 | Weather-resistant intermediate-temperature curing epoxy resin adhesive and preparation method thereof |
| CN115368857B (en) * | 2022-08-23 | 2024-07-05 | 书香门地集团股份有限公司 | Anti-cracking low-halogen high-transparency epoxy resin sealing adhesive |
| CN119529725A (en) * | 2025-01-23 | 2025-02-28 | 天津德高化成新材料股份有限公司 | Fluorescent epoxy adhesive film for epoxy CSP lamp beads and preparation method and application thereof |
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